CN103484248A - Tea flower essence with fresh and sweet characteristics, and application of essence in cigarettes - Google Patents
Tea flower essence with fresh and sweet characteristics, and application of essence in cigarettes Download PDFInfo
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Abstract
The invention provides tea flower essence with fresh and sweet characteristics, and application of the essence in cigarettes. The tea flower essence with fresh and sweet characteristics is prepared by the following steps: using a tea flower extract as primary flavor and a certain amount of a coordination agent, a modifier, a fixative and a diluent as auxiliary materials, and performing compatibility research to determine the ratio of each component so as to prepare the tea flower essence applied to the cigarettes. The tea flower essence provided by the invention has prominent fresh and sweet taste and has durable and stable fragrance. After the tea flower essence is added to the cigarettes, the fresh and sweet characteristics are given to the cigarettes, the fresh and sweet taste in the cigarette fragrance is obviously increased, and the smoking quality and the sensory comfort of the cigarettes are obviously improved.
Description
Technical field
The invention belongs to the tobacco spice technical field, relate to a kind of have the Tea Flower essence of fresh and sweet fragrant feature and the application in cigarette thereof.
Background technology
Essence and flavoring agent is widely used in the fields such as tobacco, food, daily use chemicals, and natural perfume forms complexity due to it, and fragrance is abundant, fragrance remaining time is the indispensable raw material of preparing essence lastingly.
Essence and flavoring agent not only can be given cigarette product individual style feature, also can improve cigarette jealous, is one of important connotation of constructing the Chinese-style cigarette core competitiveness.Still there is certain deficiency in current domestic cigarette product at aspects such as flavouring essence quality and sense organ comfort levels, and the exploitation of novel cigarette additive is an important solution route.Vast territory and abundant resources in China, and natural resource are of a great variety, and the composition of contained effective constituent also respectively has characteristics, for the exploitation of cigarette additive provides rich in natural resources.Can extract separation to its effective constituent by the different modes method, and for the characteristics of cigarette product, extract is applied in cigarette by blending, to improve the overall quality of cigarette.
Tea Flower is the flower of Theaceae Camellia Plants tea tree (Camellia sinensis).Tea Flower is wide at China's distributed pole, be September to next year 1, February tea tree flowering period in most of tea district, Tea Flower is a kind of without plantation cultivation, abundant and reproducible natural resource, for a long time, the tea grower only plucks the fresh and tender bud-leaf of tea tree, let alone to run its course for Tea Flower, seldom be used.
Result of study shows: fresh just exhibition Tea Flower aroma component is mainly aromatic alcohol, terpene alcohols, aliphatic alcohols and aromatic ketone compounds, and these a few class materials account for 84.1～95.6% of essential oil total content.The aroma component that its content is higher is divided into two classes according to the contribution to its odor type: a class, for bring the compound of blue or green gas to Tea Flower, comprises 2-amylalcohol, 2-enanthol, leaf alcohol, 3-amylalcohol, 1-POL, 2-hexanol etc.; Another kind of for bring the compound of the fresh and sweet fragrance of a flower (or fruital) to Tea Flower, comprise methyl phenyl ketone, phantol, methyl phenyl carbinol, 2 phenylethyl alcohol, Geraniol, wintergreen oil etc.The key odorant composition that wherein methyl phenyl ketone, methyl phenyl carbinol, 2-amylalcohol, 2 phenylethyl alcohol, phantol are Tea Flower.With the fragrant and sweet type fresh flower such as rose, compare, Tea Flower fragrance is more aobvious salubrious.Analyze reason from its fragrance composition aspect, the main aroma of finding rose is to be contributed by the terpenol of the sweet perfume (or spice) of tool and Ester thereof.Its key odorant composition is geraniol and manthanoate, acetic ester, vernol, farnesol and acetic ester, the manthanoate etc. with sweet perfume (or spice), and the existence of these compositions makes rose fragrance sweet and pure strong.And in Tea Flower, the bright refreshing fragrance of a flower aroma components of delicate fragrance such as blue or green fragrant aliphatic alcohols material and methyl phenyl ketone, phantol, methyl phenyl carbinol are more, and the content of sweet and pure strong fragrance of a flower fragrance is few, so the tea tree fragrance of a flower is fresh and sweet pleasant.
Tea Flower not only contains fresh and sweet uniqueness, pleasant aroma substance, also contain abundant polysaccharide, polyphenol, flavones isoreactivity composition, can from its essential oil, become to assign to allocate various essence and flavoring agents by separating natural, these materials or component all may have the effect that improves cigarette smoking quality to some extent.Natural plant extracts is widely used at Field of Tobacco at present, and the application of Tea Flower essence in cigarette have not been reported.
The objective of the invention is to take the Tea Flower extract as type-odor by blending, be aided with certain blender, modifier, fixative and thinner, by Study on compatibility, determine the ratio of each component, thereby mix the Tea Flower essence with fresh and sweet fragrant feature, and it is applied in cigarette.
Summary of the invention
A first aspect of the present invention provides a kind of Tea Flower essence, and this essence comprises type-odor, blender, modifier, fixative and thinner, wherein:
Described type-odor is the Tea Flower extract, and in weight part, its content is 5-30 part;
Described blender is selected from methyl phenyl ketone, phantol, phenylethyl alcohol, Dihydrojasmone, methyl dihydrojasmonate or its combination, and in weight part, its content is 0.2-0.8 part;
Described modifier is selected from caryophyllene oxide, β-caryophyllenol, β-Tujue's ketenes, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide or its combination, and in weight part, its content is 0.2-0.8 part;
Described fixative is selected from Peru's medicinal extract, Tolu concrete, aglaia odorata flower concrete, yunyan extract, tobacco extract, phenylethyl phenylacetate, benzyl cinnamate or its combination, and in weight part, its content is 5-8 part;
Described thinner is selected from propylene glycol, 95% ethanol or its combination, and in weight part, its content is 61.1-90.0 part.
According to the described Tea Flower essence of first aspect present invention, in a specific embodiment, wherein said Tea Flower extract is selected from Tea Flower medicinal extract, essential oil of the flower of Camellia sinensis, Tea Flower absolute oil, camellia tree flower tincture or its combination.
According to the described Tea Flower essence of first aspect present invention, in a specific embodiment, the flower that wherein said Tea Flower is any Theaceae Camellia Plants tea tree (Camellia sinensis).
According to the described Tea Flower essence of first aspect present invention, the preparation method of wherein said Tea Flower medicinal extract, Tea Flower absolute oil and/or Tea Flower tincture comprises the step of the raw material Tea Flower being carried out to the ultra-high voltage extraction.
According to the described Tea Flower essence of first aspect present invention, in a specific embodiment, the preparation method of the Tea Flower tincture described in the present invention, Tea Flower medicinal extract and/or Tea Flower absolute oil comprises following step (1), step (1)-(2) or step (1)-(3):
(1) ultra-high voltage extracts: take a certain amount of Tea Flower and put into the ultra-high voltage extractor, the edible ethanol that adds at least 2 times of (w/w) Tea Flower weight, carry out the ultra-high voltage extraction, obtain Tea Flower tincture 1, the concentration of wherein said edible ethanol is the 20-70%(mass concentration); Preferably, the 1/5-1/10 that Tea Flower tincture 1 is concentrated into to original volume obtains Tea Flower tincture 2;
(2) prepare Tea Flower medicinal extract: the Tea Flower tincture 1 or the Tea Flower tincture 2 that obtain in step (1) are further concentrated, obtain Tea Flower medicinal extract;
(3) prepare the Tea Flower absolute oil: the Tea Flower medicinal extract obtained by a certain amount of 95% ethanol back dissolving step (2), then carry out freezing treatment (for example-10 ℃ to-20 ℃), freezing time is that 16-48h(is preferably 20-36h) then filter, concentrated, obtain the Tea Flower absolute oil.
In the present invention, freezing temperature can be-10 ℃ to-20 ℃.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), described is that adopted Tea Flower is Tea Flower fresh flower, dried flower, spray Ethanol Treatment Tea Flower, saline soak Tea Flower or alcohol immersion Tea Flower.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), add at least edible ethanol of 2-15 times of (w/w) Tea Flower weight, be preferably 2-10 doubly, 2-8 doubly, 3-8 doubly (w/w), 4-7 doubly (w/w) more preferably, for example 4 times, 5 times, 6 times or 7 times (w/w).
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), particularly, the concentration of described edible ethanol is the 20-70%(mass concentration), 20-40%, 20-50%, 40-50%, 50-70%, 20%, 30%, 40%, 50%, 60%, 70%.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), release immediately after ultra-high voltage extracts.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), the pressure of described ultra-high voltage is 150-500Mpa; Particularly, be 150-250Mpa, 150-300Mpa, 250-300Mpa, 250-350Mpa, 250-500Mpa, 300-350Mpa, 300-500Mpa, 350-500Mpa, 150Mpa, 200Mpa, 250Mpa, 300Mpa, 350Mpa, 400Mpa, 450Mpa, 500Mpa etc.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, in step (1), dwell time is 5-120min, be preferably 5-60min, 10-30min more preferably, such as 10-15min, 10-20min, 10-25min, 15-20min, 15-25min, 15-30min, 20-25min, 20-30min, 25-30min, 10min, 15min, 20min, 25min, 30min etc.
In a specific embodiment, in the preparation method of above-mentioned Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil, concentrating in step (1) or (2) can be the method that those skilled in the art know, for example suction filtration is concentrated.
According to the described Tea Flower essence of first aspect present invention, in a specific embodiment, the preparation method of wherein said essential oil of the flower of Camellia sinensis is the reduced steam distillation method.
In a specific embodiment, the preparation method of the essential oil of the flower of Camellia sinensis described in the present invention, comprise the steps:
(1) take a certain amount of Tea Flower pack into be furnished with the trapping cold-trap the decompression extraction element in;
(2) add the water of at least 5 times of Tea Flower weight, and the temperature of the water added is more than 80 ℃, at least 5min is soaked in sealing, is cooled to 30-70 ℃;
(3-1) carry out the reduced steam distillation, temperature used is identical with cooled temperature in step (2), and vacuum tightness is 1-17kpa, collects distillate;
Preferably, also comprise step (3-2): repeating step (2) and (3-1) in operation 1 time or repeatedly, and merge distillate;
(4) in the use, low polar organic solvent carries out 1 time the distillate obtained in step (3-1) or step (3-2) or repeatedly back extraction (for example 2,3,4 or 5 times, preferably 3 times), obtains stripping workshop; Stripping workshop is concentrated, obtained enriched material;
(5) use enriched material weight 2-4 dehydrated alcohol doubly to carry out backwash to the enriched material obtained in step (4), concentrating under reduced pressure remove wherein residual in after low polar organic solvent essential oil of the flower of Camellia sinensis.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, described in step (1), be that adopted Tea Flower is Tea Flower fresh flower, dried flower, spray Ethanol Treatment Tea Flower, saline soak Tea Flower or alcohol immersion Tea Flower.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, the 5-50 that the amount of the water added in step (2) is Tea Flower weight doubly, be preferably 5-40 times or 8-40 times, more preferably 10-30 doubly, for example 10-15 doubly, 10-20 doubly, 10-25 doubly, 15-20 doubly, 15-25 doubly, 15-30 doubly, 20-25 doubly, 20-30 doubly, 10 times, 11 times, 12 times, 13 times, 14 times, 15 times, 16 times, 17 times, 18 times, 19 times, 20 times, 21 times, 22 times, 23 times, 24 times, 25 times, 26 times, 27 times, 28 times, 29 times or 30 times.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, the temperature of the water added in step (2) is preferably more than 85 ℃, more preferably more than 90 ℃, more preferably more than 95 ℃, for example 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃, preferably 100 ℃; Particularly preferably, the water added is boiling water.Be immersed under normal pressure and carry out, the temperature of the boiling water of immersion is generally 100 ℃, and those skilled in the art know, according to atmospheric difference, boiling point is different.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, the time that in step (2), sealing is soaked is 5min-4h, be preferably 5min-4h, 5min-3h or 5min-2h, more preferably 5-60min, 5-50min or 5-40min, be particularly preferably 5-30min, for example 5-18min, 5-20min, 5-25min or 18-30min.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, step is cooled to 30-70 ℃ in (2), for example 30-40 ℃, 30-50 ℃, 30-60 ℃, 40-50 ℃, 45-55 ℃, 40-60 ℃, 40-70 ℃, 50-60 ℃, 50-70 ℃ or 60-70 ℃.
Those skilled in the art know, and vacuum tightness is corresponding to a certain extent with distillation temperature, need to guarantee to allow distilled water and aroma component in matrass steam under giving fixed temperature and vacuum tightness.
Be not limited to theoretical restriction, temperature is lower, and required vacuum tightness is less, and temperature is higher, and required vacuum tightness is larger.Inventor's discovery, when temperature is 30 ℃, vacuum tightness 2.5kpa; Can be faster than the little speed distilled of 2.5kpa; When temperature is 70 ℃, vacuum tightness 17kpa; Can be faster than the little speed distilled of 17kpa.
Be not limited to theoretical restriction, on the other hand, under the prerequisite of Temperature Setting, if vacuum tightness is too low, may cause bumping, make to extract pot liquid and go out; If vacuum tightness is too high, may make to extract the pot liquid distillation not out, do not have the effect of underpressure distillation.Therefore, the corresponding proper vacuum ranges of each temperature value.
Therefore, about step (3-1) or the vacuum tightness of reduced steam (3-2) distillation, those skilled in the art can be set according to the theory above selected temperature reference or this area knowledge, also can be with reference to following vacuum ranges, or adjusted on this basis:
For example 1-12kPa, 1-10kPa, 1-9.5kPa, 1-9kPa, 1-8.5kPa, 1-8kPa, 1-7.5kPa or 1-7kPa, 2.5-7kPa for example, 1-2kPa, 1-3kPa, 1-4kPa, 1-5kPa, 1-6kPa, 2-3kPa, 2-4kPa, 2-5kPa, 2-6kPa, 2-7kPa, 3-4kPa, 3-5kPa, 3-6kPa, 3-7kPa, 4-5kPa, 4-6kPa, 4-7kPa, 5-6kPa, 5-7kPa, 6-7kPa, 6-12kPa, 8-12kPa, 10-12kPa, 1kPa, 2kPa, 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, 10kPa, 11kPa or 12kPa.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, in step (4), described in low polar organic solvent be to be selected from any one in anhydrous diethyl ether and ethyl acetate; Ethyl acetate.In described, the consumption of low polar organic solvent can be the 1/4-1/3 of distillate volume.
In a specific embodiment, in the preparation method of above-mentioned essential oil of the flower of Camellia sinensis, the decompression extraction element used can be to be commercially available, or preferably uses the decompression extraction element in the Chinese patent application that publication number is 101920127A (application number is 200910111996.2).
In a preferred embodiment of the present invention, the described Tea Flower essence of first aspect present invention any one, is characterized in that following a) to e) in any one or more:
A) described Tea Flower extract chosen from Fe kwan-yin Tea Flower medicinal extract, Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis, Chinese cassia tree Tea Flower tincture, narcissus tea tree extrait or its combination;
B) described blender, in weight part, its content is 0.2-0.4 part, 0.4-0.7 part or 0.3-0.8 part;
C) described modifier, in weight part, its content is 0.2-0.8 part, 0.3-0.5 part or 0.3-0.6 part;
D) described fixative, in weight part, its content is 5-8 part, 7-8 part or 6-6.5 part;
E) described thinner, in weight part, its content is 80.8-90.0 part, 80.6-89.8 part or 61.1-72.9 part.
In a preferred embodiment of the present invention, the described Tea Flower essence of first aspect present invention any one, it contains following composition, and its content is in weight part,
Tie Guanyin tea plant flower concrete 5-10 part, be preferably 5 parts or 10 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
β-caryophyllenol 0.1-0.4 part, be preferably 0.1 part, 0.2 part or 0.4 part;
β-ketenes the 0.1-0.4 of Tujue part, be preferably 0.1 part, 0.2 part or 0.4 part;
Peru medicinal extract 5-8 part, be preferably 5 parts or 8 parts;
Propylene glycol 25-30 part, be preferably 25 parts or 30 parts;
95% ethanol 55-60 part, be preferably 55.8-59.6 part, more preferably 55.8 parts, 56.2 parts, 59.2 parts or 59.6 parts.
In another preferred embodiment of the present invention, the described Tea Flower essence of first aspect present invention any one, it contains following composition, and its content is in weight part,
Narcissus tea tree extrait 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Tie Guanyin tea plant flower concrete 5-10 part, be preferably 5 parts or 10 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.2-0.3 part, be preferably 0.3 part or 0.2 part;
Methyl dihydrojasmonate 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
β-ketenes the 0.2-0.3 of Tujue part, be preferably 0.2 part or 0.3 part;
Oxidation isophorone 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Aglaia odorata flower concrete 2-3 part, be preferably 2 parts or 3 parts;
Yunyan extract 4-6 part, be preferably 5 parts;
Propylene glycol 25-30 part, be preferably 25 parts or 30 parts;
95% ethanol 55-60 part, be preferably 55-58 part or 56-57.2 part, more preferably 56 parts, 55.6 parts, 56.9 parts or 57.2 parts.
In another preferred embodiment of the present invention, the described Tea Flower essence of first aspect present invention any one, it contains following composition, and its content is in weight part,
Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis 0.1-0.5 part, be preferably 0.1 part or 0.5 part;
Chinese cassia tree Tea Flower tincture 20-30 part, be preferably 20 parts or 30 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Methyl phenyl ketone 0.1-0.4 part, be preferably 0.1 part or 0.2 part or 0.1 part;
β-ketenes the 0.1-0.2 of Tujue part, be preferably 0.1 part or 0.2 part;
Alpha, beta-lonone 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Dihydroactinidiolide 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Benzyl cinnamate 1-1.5 part, be preferably 1 part or 1.5 parts;
Tolu concrete 4-6 part, be preferably 5 parts;
Propylene glycol 20-30 part, be preferably 25 parts;
95% ethanol 35-50 part, be preferably 36-48 part, more preferably 36.1 parts, 37 parts, 46.5 parts or 47.9 parts.
The described Tea Flower essence of first aspect present invention any one can be used as cigaret additive, particularly as the purposes of cigarette flavors.The addition manner of this essence is: the 0.01-0.1% by pipe tobacco weight weighs up described Tea Flower essence, then with 70% alcohol dilution to 1% of pipe tobacco weight, more evenly be sprayed onto on pipe tobacco.
A second aspect of the present invention provides the purposes of Tea Flower essence in cigarette of first aspect present invention any one, preferably as the purposes of cigaret additive, particularly preferably as the purposes of cigarette flavors;
Preferably, this Tea Flower essence can be for the internal lining paper of pipe tobacco, thin slice, cigarette, filter stick etc.
A third aspect of the present invention provides a kind of cigarette, and it comprises the described Tea Flower essence of first aspect present invention any one.
Another object of the present invention is to provide the concocting method of this Tea Flower essence, take the Tea Flower extract as type-odor, be aided with certain blender, modifier and fixative, pass through Study on compatibility, determine the ratio of each component, thereby mix the Tea Flower essence with fresh and sweet fragrant feature.
Detailed Description Of The Invention
The various terms and the phrase that in the present invention, use have the general sense of well known to a person skilled in the art, but special definition is arranged in this article, with implication as defined herein, is as the criterion.
In the present invention, " tea tree " in described " Tea Flower ", if not otherwise specified, refer to the plant of Theales (Theales), Theaceae (Theaceae) or Camellia (Camellis);
In one aspect of the invention, " flower " in described " Tea Flower " comprising: perianth, androecium, gynoecium.Perianth comprises: calyx (being comprised of sepal), corolla (being comprised of petal).The color of flower and fragrance are from corolla.Stamen comprises: filigree and flower pesticide.Gynoecium comprises: column cap, style and ovary.
In one aspect of the invention, term " Tea Flower ", can be fresh flower, can be also dry flower; If there is no specified otherwise, it refers to the part of complete Tea Flower or Tea Flower; It at least comprises petal; Alternatively, also comprise and be selected from one or more in sepal, stamen and gynoecium.
In the present invention, described Tea Flower extract includes but not limited to: essential oil of the flower of Camellia sinensis, Tea Flower tincture, Tea Flower medicinal extract and/or Tea Flower absolute oil; Alternatively, it also comprises auxiliary material (carrier, solvent, pigment, antioxidant, sanitas, humectant, sweetener etc.).
Tea Flower described in the present invention extracts can pass through the normal temperature lixiviate, heating and refluxing extraction, Soxhlet is extracted, ultrasonic auxiliary extraction, microwave auxiliary extraction, the enzyme process auxiliary extraction, accelerated solvent extraction, supercritical fluid extraction, the while distillation extraction, wet distillation, the combination of any one or a few method of underpressure distillation etc. is prepared from, also can (for example: Australia China reaches spices science and technology (Guangzhou) company limited by commercially available, Huabao Edible Essence & Condiment (Shanghai), Hangzhou prompt quick essence and flavoring agent company limited, Shenzhen Bowden essence and flavoring agent company limited).
The separation method that described Tea Flower extracts can be the combination of any one or a few method of filtering separation, centrifugation, membrane sepn, molecular distillation, column chromatography, chromatographic separation etc.
Term " tincture " or " tincture " refer to uses certain density ethanol, lixiviate spice berry organ or exudate and secrete fragrant animal containing fragrant organ or its containing the resulting aroma material preparation that contains some amount ethanol of fragrant secretory product.Under normal temperature, be worth tincture to be called " cold process tincture "; The tincture made under the reflux condition is called " hot method tincture "." Tea Flower tincture " used in the present invention can, by commercially available, also can prepare by various ordinary methods.
In one embodiment of the invention, described " Tea Flower tincture " can prepare by the following method:
(1) described Tea Flower includes but not limited to fresh Tea Flower, dried flower, alcohol immersion processing Tea Flower, spray Ethanol Treatment Tea Flower etc.;
(2) ultra-high voltage extracts: take the certain quantity of fresh Tea Flower and put into the ultra-high voltage extractor, add the edible ethanol that 7 times of concentration to Tea Flower weight are 20%, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 150MPa, dwell time: 30min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains the Tea Flower tincture.
Term " essential oil ", in broad terms, essential oil refers to from spice berry and secretes the general name of the organ of fragrant animal, passing through the resulting volatility fragrant containing substance goods of processing extraction, in the narrow sense, essential oil only refers to the goods of water steam distillation method, milling process, cold grinding method or dry distillation prepared fragrant containing substance from spice berry organ (as flower, leaf, branch, skin, scapus, root, fruit, seed etc.).In actual applications, often adopt its narrow sense." essential oil of the flower of Camellia sinensis " used in the present invention can, by commercially available, also can prepare by various ordinary methods.
In one embodiment of the invention, described " essential oil of the flower of Camellia sinensis " can prepare by the following method:
(1) take the certain quantity of fresh Tea Flower and pack in the decompression extraction element, add the boiling water of 30 times of Tea Flower weight, sealing is cooled to 70 ℃ after soaking 30min;
(2) carry out the reduced steam distillation on the reliever of being furnished with the trapping cold-trap, temperature is: 70 ℃, vacuum tightness is: 12kpa, collect distillate;
(3) boiling water that 25 times of Tea Flower weight are added in underpressure distillation after complete is collected liquid to repeating twice rear merging of underpressure distillation according to step (3) in extraction element;
(4) add 0.3 times and collect the long-pending ethyl acetate back extraction of liquid three times, merge stripping workshop and be concentrated into 1/10 of fresh Tea Flower weight; ;
(5) essential oil of the flower of Camellia sinensis is refining: the dehydrated alcohol that adds 3 times of the middle concentrated solutions of step (4) carries out backwash, and concentrating under reduced pressure is removed wherein and obtained essential oil of the flower of Camellia sinensis after residual ethyl acetate.
Term " medicinal extract ", in a broad sense, medicinal extract refers to organic solvent extraction spice berry organ or its exudate (as resin, natural gum, balm), removes solvent for use and the general designation of the aroma material preparation that obtains.From narrowly, medicinal extract only refers to organic solvent extraction spice berry organ resulting not containing the aroma material preparation of solvent for use and moisture." Tea Flower medicinal extract " used in the present invention can, by commercially available, also can prepare by various ordinary methods.
In one embodiment of the invention, described " Tea Flower medicinal extract " can prepare by the following method:
(1) described Tea Flower includes but not limited to fresh Tea Flower, dried flower, alcohol immersion processing Tea Flower, spray Ethanol Treatment Tea Flower etc.;
(2) ultra-high voltage extracts: take the certain quantity of fresh Tea Flower and put into the ultra-high voltage extractor, 4 times of concentration to Tea Flower weight are 40% edible ethanol, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 500MPa, dwell time: 10min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains the Tea Flower tincture;
(4) prepare Tea Flower medicinal extract: the Tea Flower tincture continuation obtained in step (3) is concentrated and can obtain Tea Flower medicinal extract.
Term " absolute oil ", in a broad sense, refer to the solution that extracts the fragrant composition in medicinal extract, resinoid, balm or face cream with high concentration ethanol, through freezing treatment, the elimination insolubles, then after pressure reducing and steaming ethanol the general designation of the aroma material preparation of gained." Tea Flower absolute oil " used in the present invention can, by commercially available, also can prepare by various ordinary methods.
In one embodiment of the invention, described " Tea Flower absolute oil " can prepare by the following method:
(1) described Tea Flower includes but not limited to fresh Tea Flower, dried flower, alcohol immersion processing Tea Flower, spray Ethanol Treatment Tea Flower etc.;
(2) ultra-high voltage extracts: take the certain quantity of fresh Tea Flower and put into the ultra-high voltage extractor, 5 times of concentration to Tea Flower weight are 70% edible ethanol, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 300MPa, dwell time: 20min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains the Tea Flower tincture;
(4) prepare Tea Flower medicinal extract: the Tea Flower tincture continuation obtained in step (3) is concentrated and can obtain Tea Flower medicinal extract;
(5) prepare the Tea Flower absolute oil: with a certain amount of 95% ethanol back dissolving Tea Flower medicinal extract, for example, after freezing (-10 ℃ to-20 ℃) 24-48h, filter, concentrated, obtain the Tea Flower absolute oil.
(for example blender comprises methyl phenyl ketone to other spices of the present invention, phantol, phenylethyl alcohol, Dihydrojasmone, the spices such as methyl dihydrojasmonate, modifier comprises caryophyllene oxide, β-caryophyllenol, β-Tujue's ketenes, the oxidation isophorone, alpha, beta-lonone, the spices such as dihydroactinidiolide, fixative comprises Peru's medicinal extract, Tolu concrete, aglaia odorata flower concrete, yunyan extract, phenylethyl phenylacetate, the spices such as benzyl cinnamate) all can be by commercially available, for example Australia China reaches spices science and technology (Guangzhou) company limited, Huabao Edible Essence & Condiment (Shanghai), Hangzhou prompt quick essence and flavoring agent company limited, the various spices that Shenzhen Bowden essence and flavoring agent company limited provides.
The beneficial effect of the invention
Tea Flower essence provided by the invention, take the Tea Flower extract as type-odor, is aided with certain blender, modifier and fixative, by Study on compatibility, determines the ratio of each component, thereby mix the Tea Flower essence with fresh and sweet fragrant feature.This essence can be applied in cigarette.
Sensory evaluating smoking's result shows: Tea Flower essence provided by the invention, and its fresh and sweet note is more outstanding, and fragrance is lasting stability more.After adding Tea Flower essence of the present invention in cigarette, give cigarette fresh and sweet fragrant odour characteristics, the fresh and sweet note in cigarette flavor obviously increases, and the sucking quality of cigarette, sense organ comfort level are improved significantly.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example is only for the present invention is described, and should not be considered as limiting scope of the present invention.Unreceipted actual conditions person in embodiment, carry out according to the condition of normal condition or manufacturers's suggestion.The unreceipted person of production firm of component used, being can be by the conventional products of commercial acquisition.Tea Flower extract described in embodiment 1-3 is independently extracted by Fujian China Tobacco Industrial Co., Ltd., and other spices is provided by China precious essence and flavoring agent (Shanghai) Co., Ltd..
The Chinese cassia tree Tea Flower tincture of using in following embodiment prepares by the following method:
(1) raw material: fresh Chinese cassia tree Tea Flower;
(2) ultra-high voltage extracts: take certain quantity of fresh Chinese cassia tree Tea Flower and put into the ultra-high voltage extractor, add the edible ethanol that 7 times of concentration to Tea Flower weight are 20%, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 150MPa, dwell time: 30min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains Chinese cassia tree Tea Flower tincture.
The Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis of using in following embodiment prepares by the following method:
(1) take certain quantity of fresh Radix Campylotropis Hirtella (Herba Myrsines Africanae) Tea Flower and pack in the decompression extraction element, add the boiling water of 30 times of Tea Flower weight, sealing is cooled to 70 ℃ after soaking 30min;
(2) carry out the reduced steam distillation on the reliever of being furnished with the trapping cold-trap, temperature is: 70 ℃, vacuum tightness is: 12kpa, collect distillate;
(3) boiling water that 25 times of Tea Flower weight are added in underpressure distillation after complete is collected liquid to repeating twice rear merging of underpressure distillation according to step (3) in extraction element;
(4) add 0.3 times and collect the long-pending ethyl acetate back extraction of liquid three times, merge stripping workshop and be concentrated into 1/10 of fresh Tea Flower weight; ;
(5) essential oil of the flower of Camellia sinensis is refining: the dehydrated alcohol that adds 3 times of the middle concentrated solutions of step (4) carries out backwash, and concentrating under reduced pressure is removed wherein and obtained the Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis after residual ethyl acetate.
The Tie Guanyin tea plant flower concrete of using in following embodiment prepares by the following method:
(1) raw material: fresh Tie Guanyin tea plant flower;
(2) ultra-high voltage extracts: take certain quantity of fresh Tie Guanyin tea plant flower and put into the ultra-high voltage extractor, 4 times of concentration to Tea Flower weight are 40% edible ethanol, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 500MPa, dwell time: 10min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains the Tea Flower tincture;
(4) prepare Tea Flower medicinal extract: the Tea Flower tincture continuation obtained in step (3) is concentrated and can obtain the Tie Guanyin tea plant flower concrete.
The narcissus tea tree extrait of using in following embodiment prepares by the following method:
(1) raw material: fresh narcissus Tea Flower;
(2) ultra-high voltage extracts: take certain quantity of fresh narcissus tea Tea Flower and put into the ultra-high voltage extractor, 5 times of concentration to Tea Flower weight are 70% edible ethanol, carry out release immediately after the ultra-high voltage extraction; The pressure of described ultra-high voltage is: 300MPa, dwell time: 20min;
(3) the 1/5-1/10 that the extract in step (2) is carried out after suction filtration being concentrated into original volume obtains narcissus Tea Flower tincture;
(4) prepare Tea Flower medicinal extract: the Tea Flower tincture continuation obtained in step (3) is concentrated and can obtain narcissus tea tree flower concrete;
(5) prepare the Tea Flower absolute oil: with a certain amount of 95% ethanol back dissolving Tea Flower medicinal extract, for example, after freezing (-10 ℃ to-20 ℃) 24-48h, filter, concentrated, obtain narcissus tea tree extrait.
Embodiment 1
According to the formula in table 1-1, each component is mixed, prepare the Tea Flower essence with fresh and sweet fragrant feature.Wherein 1# essence in contrast, only contains a kind of Tie Guanyin tea plant flower concrete and thinner.
Table 1-1 Tea Flower perfume formulation
The fresh and sweet note of the 1# described in his-and-hers watches 1-1～5# Tea Flower essence and hold fragrant ability and carry out the Wen Xiang judgement.The Wen Xiang judgement adopts smells the mode of distinguishing, the evaluation number is 13 people, and concrete result of determination is as shown in table 1-2:
Table 1-2 Tea Flower essence is heard fragrant result of determination
By table, 1-2 can find out, the fresh and sweet note of 2#, 3#, 4#, 5# Tea Flower essence and hold fragrant ability and all be better than 1# essence, the wherein fresh and sweet note of 4# Tea Flower essence and hold fragrant ability and behave oneself best.
Hearing fragrant result of determination shows: 2#, 3#, 4#, 5# Tea Flower essence after allotment, and its fresh and sweet note is more outstanding, and fragrance is lasting stability more.
1# described in table 1-1～5# Tea Flower essence is applied to respectively in cigarette shreds, then makes cigarette and carry out cigarette flavor feature and aesthetic quality's evaluation of effect.Specific practice is: weigh up respectively the 1# of table described in 1-1～5# Tea Flower essence by 0.1% of pipe tobacco weight, then with 70% alcohol dilution to 1% of pipe tobacco weight, more evenly be sprayed onto on pipe tobacco; Wherein, blank sample applies 70% ethanolic soln by 1% of pipe tobacco weight.Aesthetic quality's evaluation of effect adopts GB5606.4-2005 " cigarette the 4th part: sense organ technical requirements ", and the evaluation number is 13 people, and concrete evaluation result is as shown in table 1-3 and table 1-4.
Table 1-3 cigarette flavor characteristic evaluating result
By table, 1-3 can find out, apply the cigarette sample of 2#, 3#, 4#, 5# Tea Flower essence, the fresh and sweet fragrant feature in its fragrance all is better than 1# and blank sample, and the fresh and sweet fragrant feature performance of 4# sample is the strongest.
Table 1-4 Sensory Quality of Cigarette evaluation result (GB5606.4-2005)
By table, 1-4 can find out, apply the cigarette sample of 2#, 3#, 4#, 5# Tea Flower essence, aesthetic quality's score is all higher than 1# and blank sample, and every quality index all is improved.
Cigarette flavor feature and aesthetic quality's evaluation of effect result show: after adding 2#, 3#, 4#, 5# Tea Flower essence in cigarette, can give cigarette fresh and sweet odour characteristics, effectively improve sucking quality and the sense organ comfort level of cigarette.
Embodiment 2
According to the formula in table 2-1, each component is mixed, prepare the Tea Flower essence with fresh and sweet fragrant feature.Wherein 6# essence in contrast, only adds Tie Guanyin tea plant flower concrete, narcissus tea tree extrait and thinner.
Table 2-1 Tea Flower perfume formulation
The fresh and sweet note of the 6# described in his-and-hers watches 2-1～10# Tea Flower essence and hold fragrant ability and carry out the Wen Xiang judgement.The Wen Xiang judgement adopts smells the mode of distinguishing, the evaluation number is 13 people, and concrete result of determination is as shown in table 2-2:
Table 2-2 Tea Flower essence is heard fragrant result of determination
By table, 2-2 can find out, the fresh and sweet note of 7#, 8#, 9#, 10# Tea Flower essence and hold fragrant ability and all be better than 6# essence, the wherein fresh and sweet note of 8# Tea Flower essence and hold fragrant ability and behave oneself best.
Hearing fragrant result of determination shows: 7#, 8#, 9#, 10# Tea Flower essence after allotment, and its fresh and sweet note is more outstanding, and fragrance is lasting stability more.
6# described in table 2-1～10# Tea Flower essence is applied to respectively in cigarette shreds, then makes cigarette and carry out cigarette flavor feature and aesthetic quality's evaluation of effect.Specific practice is: weigh up respectively the 6# of table described in 2-1～10# Tea Flower essence by 0.05% of pipe tobacco weight, then with 70% alcohol dilution to 1% of pipe tobacco weight, more evenly be sprayed onto on pipe tobacco; Wherein, blank sample applies 70% ethanolic soln by 1% of pipe tobacco weight.Aesthetic quality's evaluation of effect adopts GB5606.4-2005 " cigarette the 4th part: sense organ technical requirements ", and the evaluation number is 13 people, and concrete evaluation result is as shown in table 2-3 and table 2-4.
Table 2-3 cigarette flavor characteristic evaluating result
By table, 2-3 can find out, apply the cigarette sample of 7#, 8#, 9#, 10# Tea Flower essence, the fresh and sweet fragrant feature in its fragrance all is better than 6# and blank sample, and the fresh and sweet fragrant feature performance of 8# sample is the strongest.
Table 2-4 Sensory Quality of Cigarette evaluation result (GB5606.4-2005)
By table, 2-4 can find out, apply the cigarette sample of 7#, 8#, 9#, 10# Tea Flower essence, aesthetic quality's score is all higher than 6# and blank sample, and every quality index all is improved.
Cigarette flavor feature and aesthetic quality's evaluation of effect result show: after adding 7#, 8#, 9#, 10# Tea Flower essence in cigarette, can give cigarette fresh and sweet odour characteristics, effectively improve sucking quality and the sense organ comfort level of cigarette.
Embodiment 3
According to the formula in table 3-1, each component is mixed, prepare the Tea Flower essence with fresh and sweet fragrant feature.Wherein 11# essence in contrast, only adds Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis, Chinese cassia tree Tea Flower tincture and thinner.
Table 3-1 Tea Flower perfume formulation
The fresh and sweet note of the 11# described in his-and-hers watches 3-1～15# Tea Flower essence and hold fragrant ability and carry out the Wen Xiang judgement.The Wen Xiang judgement adopts smells the mode of distinguishing, the evaluation number is 13 people, and concrete result of determination is as shown in table 3-2:
Table 3-2 Tea Flower essence is heard fragrant result of determination
By table, 3-2 can find out, the fresh and sweet note of 12#, 13#, 14#, 15# Tea Flower essence and hold fragrant ability and all be better than 11# essence, the wherein fresh and sweet note of 14# Tea Flower essence and hold fragrant ability and behave oneself best.
Hearing fragrant result of determination shows: 12#, 13#, 14#, 15# Tea Flower essence after allotment, and its fresh and sweet note is more outstanding, and fragrance is lasting stability more.
11# described in table 3-1～15# Tea Flower essence is applied to respectively in cigarette shreds, then makes cigarette and carry out cigarette flavor feature and aesthetic quality's evaluation of effect.Specific practice is: weigh up respectively the 11# of table described in 3-1～15# Tea Flower essence by 0.01% of pipe tobacco weight, then with 70% alcohol dilution to 1% of pipe tobacco weight, more evenly be sprayed onto on pipe tobacco; Wherein, blank sample applies 70% ethanolic soln by 1% of pipe tobacco weight.Aesthetic quality's evaluation of effect adopts GB5606.4-2005 " cigarette the 4th part: sense organ technical requirements ", and the evaluation number is 13 people, and concrete evaluation result is as shown in table 3-3 and table 3-4.
Table 3-3 cigarette flavor characteristic evaluating result
By table, 3-3 can find out, apply the cigarette sample of 12#, 13#, 14#, 15# Tea Flower essence, the fresh and sweet fragrant feature in its fragrance all is better than 11# and blank sample, and the fresh and sweet fragrant feature performance of 14# sample is the strongest.
Table 3-4 Sensory Quality of Cigarette evaluation result (GB5606.4-2005)
By table, 3-4 can find out, apply the cigarette sample of 12#, 13#, 14#, 15# Tea Flower essence, aesthetic quality's score is all higher than 11# and blank sample, and every quality index all is improved.
Cigarette flavor feature and aesthetic quality's evaluation of effect result show: after adding 12#, 13#, 14#, 15# Tea Flower essence in cigarette, can give cigarette fresh and sweet odour characteristics, effectively improve sucking quality and the sense organ comfort level of cigarette.
Claims (9)
1. a Tea Flower essence, this essence comprises type-odor, blender, modifier, fixative and thinner, wherein:
Described type-odor is the Tea Flower extract, and in weight part, its content is 5-30 part;
Described blender is selected from methyl phenyl ketone, phantol, phenylethyl alcohol, Dihydrojasmone, methyl dihydrojasmonate or its combination, and in weight part, its content is 0.2-0.8 part;
Described modifier is selected from caryophyllene oxide, β-caryophyllenol, β-Tujue's ketenes, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide or its combination, and in weight part, its content is 0.2-0.8 part;
Described fixative is selected from Peru's medicinal extract, Tolu concrete, aglaia odorata flower concrete, yunyan extract, tobacco extract, phenylethyl phenylacetate, benzyl cinnamate or its combination, and in weight part, its content is 5-8 part;
Described thinner is selected from propylene glycol, 95% ethanol or its combination, and in weight part, its content is 61.1-90.0 part.
2. the Tea Flower essence of claim 1, wherein said Tea Flower extract is selected from Tea Flower medicinal extract, essential oil of the flower of Camellia sinensis, Tea Flower absolute oil, camellia tree flower tincture or its combination.
3. the Tea Flower essence of claim 1, the flower that wherein said Tea Flower is any Theaceae Camellia Plants tea tree (Camellia sinensis).
4. the Tea Flower essence of claims 1 to 3 any one, is characterized in that following a) to e) in any one or more:
A) described Tea Flower extract chosen from Fe kwan-yin Tea Flower medicinal extract, Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis, Chinese cassia tree Tea Flower tincture, narcissus tea tree extrait or its combination;
B) described blender, in weight part, its content is 0.2-0.4 part, 0.4-0.7 part or 0.3-0.8 part;
C) described modifier, in weight part, its content is 0.2-0.8 part, 0.3-0.5 part or 0.3-0.6 part;
D) described fixative, in weight part, its content is 5-8 part, 7-8 part or 6-6.5 part;
E) described thinner, in weight part, its content is 80.8-90.0 part, 80.6-89.8 part or 61.1-72.9 part.
5. the Tea Flower essence of claim 1, it contains following composition, and its content is in weight part,
Tie Guanyin tea plant flower concrete 5-10 part, be preferably 5 parts or 10 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
β-caryophyllenol 0.1-0.4 part, be preferably 0.1 part, 0.2 part or 0.4 part;
β-ketenes the 0.1-0.4 of Tujue part, be preferably 0.1 part, 0.2 part or 0.4 part;
Peru medicinal extract 5-8 part, be preferably 5 parts or 8 parts;
Propylene glycol 25-30 part, be preferably 25 parts or 30 parts;
95% ethanolic soln 55-60 part, be preferably 55.8-59.6 part, more preferably 55.8 parts, 56.2 parts, 59.2 parts or 59.6 parts.
6. the Tea Flower essence of claim 1, it contains following composition, and its content is in weight part,
Narcissus tea tree extrait 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Tie Guanyin tea plant flower concrete 5-10 part, be preferably 5 parts or 10 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.2-0.3 part, be preferably 0.3 part or 0.2 part;
Methyl dihydrojasmonate 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
β-ketenes the 0.2-0.3 of Tujue part, be preferably 0.2 part or 0.3 part;
Oxidation isophorone 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Aglaia odorata flower concrete 2-3 part, be preferably 2 parts or 3 parts;
Yunyan extract 4-6 part, be preferably 5 parts;
Propylene glycol 25-30 part, be preferably 25 parts or 30 parts;
95% ethanolic soln 55-60 part, be preferably 55-58 part or 56-57.2 part, more preferably 56 parts, 55.6 parts, 56.9 parts or 57.2 parts.
7. the Tea Flower essence of claim 1, it contains following composition, and its content is in weight part,
Radix Campylotropis Hirtella (Herba Myrsines Africanae) essential oil of the flower of Camellia sinensis 0.1-0.5 part, be preferably 0.1 part or 0.5 part;
Chinese cassia tree Tea Flower tincture 20-30 part, be preferably 20 parts or 30 parts;
Phantol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Phenylethyl alcohol 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Methyl phenyl ketone 0.1-0.4 part, be preferably 0.1 part or 0.2 part or 0.1 part;
β-ketenes the 0.1-0.2 of Tujue part, be preferably 0.1 part or 0.2 part;
Alpha, beta-lonone 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Dihydroactinidiolide 0.1-0.2 part, be preferably 0.1 part or 0.2 part;
Benzyl cinnamate 1-1.5 part, be preferably 1 part or 1.5 parts;
Tolu concrete 4-6 part, be preferably 5 parts;
Propylene glycol 20-30 part, be preferably 25 parts;
95% ethanolic soln 35-50 part, be preferably 36-48 part, more preferably 36.1 parts, 37 parts, 46.5 parts or 47.9 parts.
8. the purposes of Tea Flower essence in cigarette of claim 1-7 any one, preferably as the purposes of cigaret additive, particularly preferably as the purposes of cigarette flavors;
Preferably, this Tea Flower essence can be for the internal lining paper of pipe tobacco, thin slice, cigarette, filter stick etc.
9. a cigarette, it comprises the described Tea Flower essence of claim 1-9 any one.
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| CN108691247B (en) * | 2018-03-30 | 2020-04-28 | 河南中烟工业有限责任公司 | Cigarette packaging paper capable of increasing aroma and keeping moisture and preparation method thereof |
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